CN100358809C - Method for preparing dumbbell-like particle of negative thermal expansion material ZrWMoO8 - Google Patents
Method for preparing dumbbell-like particle of negative thermal expansion material ZrWMoO8 Download PDFInfo
- Publication number
- CN100358809C CN100358809C CNB200610040201XA CN200610040201A CN100358809C CN 100358809 C CN100358809 C CN 100358809C CN B200610040201X A CNB200610040201X A CN B200610040201XA CN 200610040201 A CN200610040201 A CN 200610040201A CN 100358809 C CN100358809 C CN 100358809C
- Authority
- CN
- China
- Prior art keywords
- mixed
- acid
- mixed solution
- thermal expansion
- zrwmoo
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a method for preparing dumbbell-shaped particles of negative thermal expansion materials (ZrWMoO8), which belongs to the technical field of functional ceramic materials. Zirconium oxynitrate, ammonium tungstate and ammonium molybdate are respectively dissolved in deionized water according to the molar ratio that Zr<4+> to W<6+> to Mo<6+> equals to 2 to 1 to 1, the three kinds of solutions are evenly stirred and mixed to form a mixed solution, the mixed acid of concentrated hydrochloric acid and concentrated sulphuric acid is added to the mixed solution, and then is evenly stirred, the volume ratio of the concentrated hydrochloric acid to the concentrated sulphuric acid is from 6: 1 to 3: 1, and the volume of the mixed acid is from 1/6 to 1/3 of the volume of the mixed solution; after the mixed solution adding the mixed acid carries out reflux for 24 to 96 hours, the mixed solution is repeatedly washed by ionized water, and is baked at 50 to 80 DEG C to obtain a precursor (ZrWMoO7 (OH)2 (H2O)2). The precursor is heated at 500 to 620 DEG C for more than five hours to obtain the dumbbell-shaped particles of a final product (ZrWMoO8). The present invention has the advantages of simple procedure and easy operation.
Description
Technical field
The invention belongs to the ceramic material technical field, particularly a kind of negative thermal expansion material ZrWMoO
8Dumbbell shaped particle preparation method.
Background technology
ZrWMoO
8Be good isotropic negative heat expansion compound, (negative expansion coefficient is up to-8.7 * 10 in 0～1473K) in extremely wide temperature range
-6K
-1The maximum at present purposes of negative thermal expansion material is exactly and the positive compound preparation matrix material of thermal expansion material, thus the volume coefficient of accurate control material, and its potential Application Areas has optics, opticfiber communication, medical material, low-temperature sensor, thermopair etc.But negative thermal expansion material causes stress raisers when making matrix material with just thermal expansion material is compound easily, thereby causes the generation of tiny crack, influences its practical application.In order to reduce stress concentration, the isotropy negative thermal expansion material that preparation has regular shape has crucial meaning.Up to the present, still do not prepare dumbbell shaped ZrWMoO
8The report of particle.
Summary of the invention
The objective of the invention is to utilize circumfluence method to synthesize negative thermal expansion material ZrWMoO
8The dumbbell shaped particle.
A kind of negative thermal expansion material ZrWMoO
8Dumbbell shaped particle preparation method, adopt the synthetic negative thermal expansion material ZrWMoO of circumfluence method
8The dumbbell shaped particle.Raw materials usedly be: ZrO (NO
3)
25H
2O (analytical pure), N
5H
37W
6O
24H
2O (chemical pure), N
6H
24Mo
7O
244H
2O (chemical pure), HCl (analytical pure), H
2SO
4(analytical pure).
Preparation technology is:
(1) Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Z
4+: W
6+: Mo
6+Mol ratio is respectively to be dissolved in deionized water at 2: 1: 1, and three kinds of solution stirring are mixed, and adding concentrated hydrochloric acid and vitriol oil volume ratio to mixed solution is 6: 1～3: 1 mixing acid, and the volume of mixing acid is 1/6～1/3 of a mixeding liquid volume, and restir is even;
(2) will add after the mixed-liquor return 24-96h of mixing acid, and use the deionized water repetitive scrubbing, 50～80 ℃ of oven dry obtain presoma ZrWMoO
7(OH)
2(H
2O)
2
(3) presoma is got final product ZrWMoO in 500～620 ℃ of heating more than 5 hours
8The dumbbell shaped particle.
In the step 1 concentrated hydrochloric acid and vitriol oil volume ratio be 5: 1～4: 1 for good;
Return time 56～72h in the step 2, ageing is good more than 3 days after refluxing.
The invention has the advantages that and utilize circumfluence method to synthesize negative thermal expansion material ZrWMoO
8The dumbbell shaped particle, this method program is simple, easy handling.
Figure of description
Fig. 1 ZrWMoO
8The SEM figure of powder
Embodiment:
Embodiment 1
At first Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio is to mix at 2: 1: 1 to be dissolved in respectively in the deionized water, constantly under the stirring condition three kinds of solution is being mixed, and adding concentrated hydrochloric acid and vitriol oil volume ratio to mixed solution is 6: 1 mixing acid, and the volume of mixing acid is 1/6 of a mixeding liquid volume, stirs 12h; With mixed solution at 100 ℃ of backflow 36h.The reaction back room temperature ageing 5 days that finishes is 7 with deionized water repetitive scrubbing to pH value, drips Ag in the stillness of night respectively to the centrifugal upper strata that goes out
+Solution and Ba
+Solution does not all produce white precipitate, 50 ℃ of oven dry.Presoma is got final product dumbbell shaped ZrWMoO in 500 ℃ of heating 6h in resistance furnace
8Particle.
Embodiment 2
At first Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio is that mixing in 2: 1: 1 is dissolved in the deionized water respectively, constantly under the stirring condition three kinds of solution are being mixed, adding a certain amount of concentrated hydrochloric acid and vitriol oil volume ratio to mixed solution is 4: 1 mixing acid, and the volume of mixing acid is 1/4 of a mixeding liquid volume, stirs 24h; With mixed solution at 100 ℃ of backflow 72h.The reaction back room temperature ageing 7 days that finishes is 7 with deionized water repetitive scrubbing to pH value, drips Ag in the stillness of night respectively to the centrifugal upper strata that goes out
+Solution and Ba
+Solution does not all produce white precipitate, 60 ℃ of oven dry.Presoma is got final product dumbbell shaped ZrWMoO in 530 ℃ of heating 6h in resistance furnace
8Particle.
Embodiment 3
At first Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio is that mixing in 2: 1: 1 is dissolved in the deionized water respectively, constantly under the stirring condition three kinds of solution are being mixed, adding a certain amount of concentrated hydrochloric acid and vitriol oil volume ratio to mixed solution is 3: 1 mixing acid, and the volume of mixing acid is 1/3 of a mixeding liquid volume, stirs 24h; With mixed solution at 120 ℃ of backflow 96h.The reaction back room temperature ageing 21 days that finishes is 7 with deionized water repetitive scrubbing to pH value, drips Ag in the stillness of night respectively to the centrifugal upper strata that goes out
+Solution and Ba
+Solution does not all produce white precipitate, 80 ℃ of oven dry.Presoma is got final product dumbbell shaped ZrWMoO in 620 ℃ of heating 5h in resistance furnace
8Particle.
Claims (2)
1, a kind of negative thermal expansion material ZrWMoO
8Dumbbell shaped particle preparation method, it is characterized in that:
(1) Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio is respectively to be dissolved in deionized water at 2: 1: 1, and three kinds of solution stirring are mixed, and adding concentrated hydrochloric acid and vitriol oil volume ratio to mixed solution is 6: 1～3: 1 mixing acid, and the volume of mixing acid is 1/6～1/3 of a mixeding liquid volume, and restir is even;
(2) will add after the mixed-liquor return 24～96h of mixing acid, and use the deionized water repetitive scrubbing, 50～80 ℃ of oven dry obtain presoma ZrWMoO
7(OH)
2(H
2O)
2
(3) presoma is got final product ZrWMoO in 500～620 ℃ of heating more than 5 hours
8The dumbbell shaped particle.
2, a kind of negative thermal expansion material ZrWMoO according to claim 1
8Dumbbell shaped particle preparation method, it is characterized in that: concentrated hydrochloric acid and vitriol oil volume ratio are 5: 1～4: 1 in the step 1; Return time 56～72h in the step 2, ageing is more than 3 days after refluxing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610040201XA CN100358809C (en) | 2006-05-11 | 2006-05-11 | Method for preparing dumbbell-like particle of negative thermal expansion material ZrWMoO8 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610040201XA CN100358809C (en) | 2006-05-11 | 2006-05-11 | Method for preparing dumbbell-like particle of negative thermal expansion material ZrWMoO8 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1850610A CN1850610A (en) | 2006-10-25 |
| CN100358809C true CN100358809C (en) | 2008-01-02 |
Family
ID=37132111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200610040201XA Expired - Fee Related CN100358809C (en) | 2006-05-11 | 2006-05-11 | Method for preparing dumbbell-like particle of negative thermal expansion material ZrWMoO8 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100358809C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011022859A1 (en) * | 2009-08-27 | 2011-03-03 | 江苏大学 | PROCESS FOR PREPARING VARIOUS MORPHOLOGY NTE COMPOUND ZrW0.5Mo1.5O8 |
| CN102745747B (en) * | 2011-12-14 | 2014-07-30 | 江苏大学 | Preparation method for rod-like Sc2W3O12 negative thermal expansion material |
| CN104445421A (en) * | 2014-12-16 | 2015-03-25 | 湖南科技大学 | Ion-doped ZrWMoO8 complex-phase controlled expansion material and prepration method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5322559A (en) * | 1993-05-11 | 1994-06-21 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Negative thermal expansion material |
| US6183716B1 (en) * | 1997-07-30 | 2001-02-06 | State Of Oregon Acting By And Through The State Board Of Higher Education Of Behalf Of Oregon State University | Solution method for making molybdate and tungstate negative thermal expansion materials and compounds made by the method |
| CN1594207A (en) * | 2004-07-01 | 2005-03-16 | 上海交通大学 | Negative thermal-expansion coefficient adjustable laminated ceramic matrix composite and preparing method thereof |
| CN1680637A (en) * | 2005-01-25 | 2005-10-12 | 北京科技大学 | Preparation of single-crystal of thermal negative expanding material ZrW2O8 |
-
2006
- 2006-05-11 CN CNB200610040201XA patent/CN100358809C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5322559A (en) * | 1993-05-11 | 1994-06-21 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Negative thermal expansion material |
| US6183716B1 (en) * | 1997-07-30 | 2001-02-06 | State Of Oregon Acting By And Through The State Board Of Higher Education Of Behalf Of Oregon State University | Solution method for making molybdate and tungstate negative thermal expansion materials and compounds made by the method |
| CN1594207A (en) * | 2004-07-01 | 2005-03-16 | 上海交通大学 | Negative thermal-expansion coefficient adjustable laminated ceramic matrix composite and preparing method thereof |
| CN1680637A (en) * | 2005-01-25 | 2005-10-12 | 北京科技大学 | Preparation of single-crystal of thermal negative expanding material ZrW2O8 |
Non-Patent Citations (1)
| Title |
|---|
| 负热膨胀化合物材料ZrW_2O_8的机理与制备技术. 程晓农，张美芬，严学华.江苏大学学报(自然科学版)，第25卷第3期. 2004 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1850610A (en) | 2006-10-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100462307C (en) | Method for preparation of niobic acid zinc nano material | |
| CN106542560B (en) | A kind of preparation method of rare earth oxysulfate | |
| CN105129805B (en) | Preparation method of silicon oxide/tin antimony oxide/zinc oxide ternary composite material | |
| CN101597086A (en) | Method for preparing nano manganese dioxide with different crystal forms in low-temperature acid solution | |
| CN103058265B (en) | Preparation method of mesoporous nano flaky zinc oxide powder with high specific surface area | |
| CN101113010A (en) | Method for preparing cerium oxide nano particle by auxiliary microwave | |
| CN105329876A (en) | Preparation method of boron-nitrogen-co-doped carbon dots | |
| CN102674834A (en) | Preparation method of zirconium oxide structural ceramics | |
| CN100358809C (en) | Method for preparing dumbbell-like particle of negative thermal expansion material ZrWMoO8 | |
| CN108457000B (en) | CuO/ZnO heterostructure loaded on nanofiber membrane and preparation method thereof | |
| CN101544402B (en) | Nanometer zirconia sol and preparation method thereof | |
| CN102070178A (en) | Method for preparing yttrium oxide micro-nano-materials based on hydrothermal technology regulation and control | |
| CN101462760A (en) | Method for preparing high performance yttrium oxide material | |
| CN105905944A (en) | Method of preparing Bi2Zr2O7 nano material through non-hydrolytic sol-gel method | |
| CN100410427C (en) | Method for preparing material of ZrW1.7Mo0.308 single crystal in minus heat expansion | |
| CN1760157A (en) | A kind of preparation method of lutecia based transparent ceramics | |
| CN104192890A (en) | Method for preparing carbon-dope zinc oxide nanopillars | |
| CN106744741A (en) | A kind of Fe2O3 doping titanium nitride nano pipe and its preparation method and application | |
| CN102745747B (en) | Preparation method for rod-like Sc2W3O12 negative thermal expansion material | |
| CN106732534B (en) | A kind of infrared ray excited bismuth tungstate photocatalyst and preparation method thereof | |
| CN101921112A (en) | Sol-gel method for preparing potassium-sodium niobate nano-powder | |
| CN105753058B (en) | A kind of method that perovskite is synthesized using natural organic formwork | |
| CN109713348A (en) | It is a kind of to prepare bismuth oxide base electrolyte material Bi using the combustion-supporting method of microwave1-xAxO1.5-δMethod | |
| CN102936042A (en) | Method for preparing sheet Bi7VO13 powder with microwave hydrothermal method | |
| CN103159479A (en) | Gd2O3-modified La2Zr2O7-(Zr0.92Y0.08)O1.96 complex phase thermal barrier coating material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080102 Termination date: 20110511 |